反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
In this step, synthesis of an active ester of a binding enhancer is described, which can then be easily conjugated to both the photoreactive ligand and the linker. A solution of bisbenzimidazole (6 g, 0.01 mol) dicyclohexylcarbodiimide (0.05 mol) and succinic acid (0.01 mol) in 100 mL of chloroform is stirred overnight ( 18-24 hrs). During this time, a white precipitate is formed. The precipitate is filtered of and washed with chloroform (2×50 mL). The combined chloroform is concentrated under vacuum in a rotary evaporator and the residue purified by flash column chromatography. The fractions containing the product is combined and concentrated under vacuum in a rotary evaporate to afford bisbenzimide succinnate ester (80%) as a white solid.
WORKUP
后处理
- customDuring this time, a white precipitate is formed
- filtrationThe precipitate is filtered of and
- washwashed with chloroform (2×50 mL)
- concentrationThe combined chloroform is concentrated under vacuum in a rotary evaporator
- customthe residue purified by flash column chromatography
- additionThe fractions containing the product
- concentrationconcentrated under vacuum in
- customa rotary evaporate